Apparatus for the final concentration of oil of vitriol



(No Model.) 2 Sheets-Sheet 1.

R. S. PENNIMAN. APPARATUS TOR THE FINAL CONCENTRATION OP OIL 0F VITNIOL.

No. 469,439. i Patented Feb. 23, 1892.

Ornag.

(No Model.) 2 Sheet`s-Sheet 2.

R. S; PENNIMAN. APPARATUS TON THE FINAL CONCENTRATION 0T OIL 0T VTTRIOL.

N0. 469,439. Patented Feb.23,1892.

Inv/envo? ugorney.

mt Noam Pinus co., muroilrnc., wAsNmnYou, u. c.

NrTED STATES PATENT" OFFICE.N

RUSSELL S. PENNIMAN, OF DOVER, NEI/V JERSEY, ASSIGNOR TO THE ATLAN- TIC DYNAMITE COMPANY, OF SAN FRANCISCO, CALIFORNIA.

APPARATUS FOR THE FINAL CONCENTRATION OF OIL OF VITRIOL.

SPECIFICATION forming part of Letters Patent No. 469,439, dated February 23, 1892.

` Application iled March 15, 1886. Serial No. 195,313 (No model.)

To all whom it may concern: y acids as are liable to andfrequently exist in Be it known that I, RUSSELL S.-PENNIMAN, acids to be concentrated.l The use of iron of Dover, in the county of Morris and State retorts is more or less objectionable, because of NewJersey,haveinvented certain new and of the well-known adverse effect of the iron 55 5 useful Improvements in Apparatus for the upon the product, rendering it unfit for some Final Concentration of Oil of Vitriol; and I purposes. In both processes glass retorts i do hereby declare that the following specifihave also been used, and notwithstanding cation, taken in connection with the drawtheir capacity to resist corrosion, and to asings furnished and forming a part of the sure the integrity of the product concentrated 6o to same, is a clear, true, and complete descriptherein and the great economy involved in tion of the several features of my invention. lirst cost, their liability to breakage, and the Introductory to a statement of my invenattendant waste in acid and time and labor, tion it should be understood that the final as well as danger to attendants, has largely concentration of oil of vitriol has been hereprecluded their use in favor of the metalvre- 65 I5 tofore practiced under processes properly torts, especially in continuous-process appatermed the intermittent and the continuratus, although single glass retorts are used ons processes-in other words, by the use of to some extent under the intermittent proa single retort, which is alternately charged, cess, as a choice between two evils, in avoidoperated, cooled, and emptied in the one case, `ing the high cost of platinum retorts, and the 7o zo and in the other by the use of a series of redeteriorating effect of iron on the product torts coupled together in a descending grade, while encountering the greater cost in fuel so that as weak acid is continuously supplied and labor, as well as the liability to wastage to the highest retort it gradually flows thereand danger to attendants incident to breakfrom to the next, and so on, more or less conage. 7 5 2 5 centration being effected in each retort down It has been hereinbefore indicated that my to the lowest, from which the concentrated prime object is to obtain all of the advantages product is continuously delivered. incident to the continuous process, and I will The prime value of my improvements acnow state that it further includes the obtaincrues in connection with said continuous proing of all the advantages incident to the use 8o 3o cess, it being the main object of my invenof glass retorts, all of which practically detion to secure all of its economic advantages pend upon reducing the liability of their in the use of fuel as well as attendance and breakage to a minimum. It should next be* capacity in production, and for the first time, understood that the results of said breakage as I believe, to obtain as complete results in in the intermittent process are triiiingas corn- 85 3 5 the way of concentration as have been or can pared with the breakage of aretort in a conbe obtained on a large scale by the intermittinuous-process apparatus, because breakage tent process. In both processes retorts of vais less liable in the intermittent than in the rious kinds have been employed-as for incontinuous process and also because the one stance, they have been composed of platinum retort and its contents are alone involved in 9o 4o and of iron-according to circumstances, nothe one case, while in the continuous process tably in the continuous process, wherein platthe entire plant is crippled by the breakage inum retorts have been used for the lower of a single retort, and from, or as the result concentrations co-operatively with iron reof one breakage, other adjacent retorts are torts, which arerelied upon for the high conalso more or less liable to be broken. It 95 45 centrations. In the concentration of all sulshould be further understood that the usual phuric acid, especially that derived from pyforms of breakage with the single glass retort rites, it is well known that iron salts are deunder the intermittent process are so unlike posited in the retorts, and these are capable the usual forms of breakage in retorts coupled of more or less corrosive and destructive effor the continuous process as to clearly indiroc 5o feet upon the bottomsof the platinum recate widely-different causes. With the single torts, and the same is true of such nitrogen retort the usual breakage is a smashing ot' the bottom, as a result of what is known as bumping, caused by a sudden ebullition in mass of the contents of the retort under high temperatures. With the coupled retort in a continuous-process plant the usual breakage is on a peripheral line adjacent to the normal level of its contents, due probably to abrupt variations in expansion of the upper and lower portions of the retort incident to the gradual entry and discharge of acids, which are maintained at a non-variable level in each retort. With the coupled retort bumping seldom occurs, because of the comparatively low temperatures and the continuous iiow of the acid; but even this contingency is reduced to a minimum, and in fact is practically obviated in my approved apparatus.

Now all of the desirable ends stated are attained by me, because I have, as I believe, for the first time combined with the coupled glass retorts in a continuous process apparatus means for maintaining the contents of each in such a condition as to uniform temperature as to practically obviate breakage of the retorts; and I am also, so far as I know, the first to combine such means with a single glass retort used in the intermittent process for concentrating oil of vitriol. For thus equalizing the temperature of the contents of a glass retort-I rely upon agitation, and this may be variously accomplished without departure from the main feature of my invention. Good results will accrue from the use of mechanically-operated stirring contrivances within the retort. Better results will accrue from the use of injected air operating mechanically as an agitating medium if 'the air be properly controlled and applied; but the best results will accrue from the use of a mechanicallydriven stirrer in conjunction with injected air under proper conditions. The agitation of the contents of a series of glass retorts in a continuous-process apparatus as practiced by me is also of practical value, in that it results in preventing the undue deposit of salts in the retorts, as well as in the connectingtubes, wherein obstruction is well known to be liable to occur as a result of such deposits.

Inasniuch as it appears from the aforesaid statement of the means for agitation relied upon by me thatinjected air under proper conditions is, when broadly considered, an equivalent for a mechanically constructed and operated stirring contrivance, it is believed to be proper to next refer to certain prior uses of injected air for enabling a bet-` ter understanding of the status of my invention iu the art of manufacturing sulphuric acid, and especially in that particular part thereof which embraces the final concentration of oil of vitriol, it being of course understood that the acids to be supplied to a concentrating plant are such as have been manufactured by methods which need only involve the use of such well-known apparatus as in no manner pertains to my invention.

In the manufacture ot' sulphuric acid open pans of lead yor other metal have been employed, and into the contents of said pans air has been liberally injected; butit will be obvious that the results of said prior use of air are in no manner pertinent to the protection of glass retorts.

In the purification of sulphur-ic acid or oil of vitriol single glass retorts have been employed and air has been injected therein; but this process differs from the process of concentration, in that in said purication process the-product sought is carried over from and out of the retort, while in the concentration process the product sought is retained in the retort. Moreovenin the purification process higher temperatures are involved than are usual in concentration. In the purifying process air was injected into said single retort solely for the purpose ofl facilitating the upward passage of vapors from the highlyheated portions of the surface of the retort, and thereby preventing bumping by obviating sudden ebullition in mass, and as equiva lents of the injected air platinum scraps or wire, or bits of quartz, or of porcelain, or of hard coke have been placed in the retorts and successfully relied upon for so assembling and controlling the vapors evolved at the bottom of the retort as to prevent bumping. Now when it is considered that bumping is a remote contingency in a concentrating-retort, and that neither one nor all of said solid bodies heretofore introduced will serve my purposes, it should be obvious that the said prior use of injected air into asingle glass retort used for purication is distinct and separate from the use of injected air by me as an agitating medium in a glass retort used for concentration, and especially in a series of glass retorts in an apparatus for concentration by the continuous process for the purpose of preventing the prevailing peripheral breakage. In the use of air as by me, however, the vapors eliminated within the retort are more readily discharged than when a niey chanical stirrer is alone employed, and to this extent air injected into a concentrating-retort would serve the same purpose as when injected intoa retort used for purification, and it is for that reason thatI prefer injected air, whether as the sole or a co-operative means of agitation.

An apparatus embodying my invention in a desirable form has been extensively operated and tested by me with thoroughly satisfactory results, and said apparatus is illustrated in my drawings with such variations therein as will best illustrate theseveral features of my invention, all of which after a description of details will be duly specified in the several clauses of the claim hereunto annexed.

Referring to the two sheets of drawings, Figure l is a side elevation of my apparatus in a practically desirable form. Fig. 2 is a sectional view of a detached retort with its immediate coupling connections as organized IOO IIO

when injected air is alone relied upon for agitation. Fig. 3 is a view similar to Fig. 2, illustrating a mechanical stirrer or agitator within a retort and lin a form well adapted for use with or without injected air. Fig. l is a top or planvview of the mechanism for operating the stirrer shown in Fig. 3. Fig. 5 is a View similar to Fig. 2illustrating a rotating mechanical stirrer, also adapted to be used with or without injected air. Fig. G is a portion of an air-injecting pipe in section for illustrating a perforated diaphragm as used by me.

In Fig. l neither the fire-box nor heating flue is disclosed, and it is to be understood that any desired variations may be made therein without departure from the main feature of my invention. The uptake or chimney is not shown; but it is to be understood that ample draft for the furnace should be provided.

The glass retorts A are of a well-known form, and in the usual manner they are supported in sand baths within iron kettles. The number of retorts in an apparatus may be varied; but I prefer to employ twelve in each series, as shown, and I mount them in the masonry with relation to each other, so as to fairly economize space and allow a descending grade between each two of about six inches. As heretofore, each retort has pipeholes on its upper and lower sides for enabling them te be coupled together, as shown, by means of the pipes d, which are preferably composed of glass, although other materials well known to be suitable may be employed. The lowest retort of the series discharges the concentrated product by way of pipe a into a suitable tank or cooler a2. Tl'i'e neck of each retort is coupled by means of the usual alembic head b to an inclined trunk or conduit c, communicating at its upper end with the same uptakeor chimney which the retort-flue enters. The trunk c, as heretofore, receives the liquid products of condensation,

which flow downward and are discharged" from itslowerend. Each alembic head above the neck of its retort is provided with an aperture large enough to loosely receive the glass tube d, which, as shown in Fig. 2, has a rubber collar and is suspended from a rail c, provided with holes, and each pipe is so supported that its lower end will be about one inch above the bottom of the retort. Each glass tube is connected by a pipe of tiexible tube d with a metal pipef, and these latter communicate with a compressed-air receiver B by way of the main pipe g, which is provided with a pressure-gage g. It is vitally important that there be interposed between many cases power may as well be derived from a motor, also relied upon for other Vpurposes.

It will be seen that each pipef is provided with a cock 7i; but this is really of consequence only for cutting oi communication entirely, and should seldom, if ever, be relied upon for graduation.

In the main pipe g, nearthe receiver, I employ a reliable pressure regulator D of any of the well-known eflicient types, and this needs no specific description. For obtaining the best results I have adjusted my regulator, so that regardless of the pressure within the receiver air will be delivered into the distributing-pipes f at a pressure of about live pounds to the inch and in the receiver I range with, say, from fifty pounds downward to about ten pounds. y

As a result of my experimenting as to the volume of air injected into the retorts, I deem it undesirable tovinject more air than will afford the degree of agitation essential to sec-ure a practically uniform temperature throughout the contents of a retort. However much the air may be heated as a result of compression or from the ordinary temperature of the space traversed by the pipes, it is injected into a more or less highly-heated body of acid within a retort, and its volume is thereby suddenly increased by expansion, and hence if the quantity of air to be injected be not accurately determined and the injection evenly controlled the objects sought by me will be defeated. Even with a pressure regulator of the best form known to me and with the cocks h, I experienced such difficulty in properly controlling the injection of air to the retorts as to prompt me to experiment with many additional means, and finally in finding a device which I have used with highly-satisfactory results. Between each cock l1, and connected glass tube I introduce a metal diaphragm t', as shown in Fig. 6, which is provided with a single central perforation. With pressure at from, say, three to tive pounds in the pipe g, I found that when said perforation was as large as a common pin the quantity of air injected was much too great; but when said hole could be filled by theA finest sewing-needle perfectly satisfactory results were obtained.

It is not to be understood that my invention is restricted to dimensions indicated or that other pressures may not be successfully employed, but that results in every way desirable will positively accrue by the use of an apparatus constructed as described and operated under the pressures indicated.

Inasmuch as the agitation of the contents of the retort is what I seek to accomplish, I

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do not limit my invention to injected air as an agitating medium.

In Fig. 3 I illustrate a desirable stirring contrivance. The pipe d here shown may serve as a pipe or asa mere rod, having Wings or arms d2 at its lower end. Instead of being suspended on a rail, as in Figs. l and 2, said pipe-rod has a suitable ball 7c fixed thereto, and which, when occupying a cup-shaped neck on the alembic head, will maintain the stirrer at a proper the retort.

For imparting motionto the stirrer asmall rotating crank-wheel Z, Fig. 4, is coupled to a reciprocating and vibrating'arm m, having at its front end a gimbal-joint n, containing a clamp which iirmlyembraces the upper end of the pipe-rod. The arm m at its rear end terminates in a tail-piece m', sliding through a hole in a pivoted guiding-head m2, so that as the crank-wheel is revolved the upper. endl of the rod is moved in a circular path and the lower end within the retort is correspondingly moved, as much as when a paddle is operated by hand Afor stirring. The non-rotation of the pipe-rod on its axis enables it to be readily coupled by flexible pipes, as` before described, to the air-pipes f; but the stirrer may be rotated, if desired, and still beA coupled to theair-pipesf-as, for instance, as illustrated in Fig. 5, wherein the pipe-rod dis suspended from a wide rail and provided with a bevel-gear o, meshed by a driving-gear. In this case the upper end of the pipe-rod d is internally tapered and a felt-cladnozzle p is fitted thereto, and at its rear end the connection with the flexible tube Clis made, 'so that when the pipe-rod is rotated the nozzle p is stationary and a reasonablytight joint secured by the felt packing without undue friction. When the agitators are organized .ff/"to operate both with and without injected air,

any accident occurring either to the air-injecting devices or to the stirring contrivances need not interfere with the agitation, because both would seldom be crippled at the sam time.

With my apparatus I have produced. as high concentrations as are ordinarily produced by the intermittent process and with point above the bottom of far greater economy, and the loss in time and retortsfrom breakage has been so slight as to constitute practically unimportant items in the cost of manufacture.

While forobtaining the best results I prefer an apparatusembodying'all of the severalseries ofv coupled glass retorts and means, substantially as described, for agitating thecon` tents ot' said retorts when heated and thereby obviating the liability of injury to said retorts by peripheral breakage.

2. In an apparatus for concentrating oil of vvitriol by continuous process, the series of glass retorts coupledtogether, in combination with pipes projecting into saidl retorts and an air-pump forinjecting air through said pipes into the contents ofsaid retorts, substantially as and forthe purposes specified.

3. In an apparatus for concentrating oil ot` vitriol by continuous process, the combination of a series of glass retorts coupled together,

pipes extending within said retorts and coupled lto an air-receiver, andv a pressure-regulator between said. receiver and the retorts, substantially as and for the purposes specified.

4. In-an apparatus for concentrating oil of vitriol bycdntinuous process, the combination,

substantially as hereinbefore described, of

the series of coupled retorts, the air-injecting pipes therein coupled by suitable pipes-to an air-receiver, the pressure-regulator, and a finely-perforated diaphragm with-in each of saidcoupling-pipes between said pressureregulator and each retort.

RUSSELLv S. PENNIMAN. Witnesses:

CHARLES H; MUNsoN, JAMES H. NEIGHBOUR. 

